The use of paper devices in chemical analysis has been increased due to their low cost, high surface area, portability, and biodegradability. A novel use of paper devices is proposed using thermal infrared enthalpimetry (TIE) for a rapid, green, and high throughput determination of wine acidities. The determination of total, fixed, and volatile acidities in red, white, and sparkling wine was carried out, and the results were compared with AOAC titration method. A multichannel pipette was used for reagent addition and an infrared camera for the temperature monitoring. The pipetting and temperature measurement conditions presented direct influence in the deviations among the measurements. The results obtained by TIE presented an agreement between 96 and 104% with the reference method (AOAC 962.12), for all samples. A high sample throughput was achieved reaching 480 samples h-1 for total acidity. A significant reduction in sample volume and reagent consumption was also obtained, with energy consumption up to 60 times lower in relation to the AOAC method. The association of TIE with a paper device provided a rapid, reliable and green method for the determination of acidities of wines.

Currently, the pharmaceutical industry devotes great attention to drug degradation products because these compounds can offer risks to patients. A previous degradation study of betahistine (N-α-methyl-2-pyridylethylamine) conducted under different stress conditions detected three main impurities named A, B and C. Degradation products were analyzed by high-resolution mass spectrometry in electrospray source and time of flight analyzer (ESI-TOF) and nuclear magnetic resonance (NMR). Impurity mutagenicity was evaluated by Derek Nexus and Sarah Nexus softwares. Liquid chromatography hyphenate with tandem mass spectrometry (LC-MS/MS) analysis of the betahistine forced degradation sample indicated the presence of a new impurity, which was named impurity C1. 2D NMR experiments allowed the complete structural characterization of the new entity. The active pharmaceutical ingredient and degradation impurities were classified as inactive in the in silico mutagenic studies. Systematic investigation of a forced degradation sample led to the characterization of a new betahistine impurity. The in silico mutagenicity study of the betahistine degradation impurities may be useful in the risk assessment of the drug products.

ABSTRACT The study of radiation entrance and exit dynamics and energy consumption in a system is important for understanding the environmental processes that rule the biosphere-atmosphere interactions of all ecosystems. This study provides an analysis of the interaction of energy in the form of photosynthetically active radiation (PAR) in the Pantanal, a Brazilian wetland forest, by studying the variation of PAR reflectance and its interaction with local rainfall. The study site is located in Private Reserve of Natural Heritage, Mato Grosso State, Brazil, where the vegetation is a monodominant forest of Vochysia divergens Phol. The results showed a high correlation between the reflection of visible radiation and rainfall; however, the behavior was not the same at the three heights studied. An analysis of the hourly variation of the reflected waves also showed the seasonality of these phenomena in relation to the dry and rainy seasons. A predictive model for PAR was developed with a neural network that has a hidden layer, and it showed a determination coefficient of 0.938. This model showed that the Julian day and time of measurements had an inverse association with the wind profile and a direct association with the relative humidity profile.

Com o objetivo de avaliar a toxicidade de diferentes concentrações das favas de Stryphnodendron fissuratum em vacas prenhes, as favas desta árvore foram moídas, misturadas à ração comercial e fornecidas a oito vacas nas doses totais de 6,5g/kg, 7,5g/kg, 9g/kg e 10g/kg. Os animais que receberam doses de 6,5g/kg pariram bezerros normais e aqueles que receberam 7,5g/kg pariram bezerros fracos que não sobreviveram. Doses de 9g/kg resultaram no nascimento de um bezerro imaturo e de outro bezerro com distiquíase, opacidade congênita das córneas e microftalmia. Ambas as vacas que ingeriram 10g/kg morreram, porém uma vaca abortou antes de morrer. Nas vacas que morreram, as lesões macroscópicas e histológicas do sistema digestivo e fígado foram semelhantes às descritas anteriormente na intoxicação por S. fissuratum. Nos bezerros e no feto abortado não foram observadas lesões macroscópicas ou histológicas significantes. A análise fitoquímica dos extratos metanólicos das favas de S. fissuratum revelou a presença de taninos hidrossolúveis, proantocianidinas, leucoantocianidinas e da saponina triterpénica β-amirina. Saponinas triterpénicas têm sido associadas com a toxicidade das favas de Stryphnodendron spp. e Enterolobium spp., que causam sinais clínicos semelhantes aos observados na intoxicação por S. fissuratum. Esta pesquisa confirmou a toxicidade das favas de S. fissuratum para bovinos, no entanto não foram confirmados os efeitos abortivos das mesmas, pois o aborto e as mortes neonatais observadas podem ser decorrentes dos efeitos tóxicos da planta nas mães. Novas pesquisas são necessárias para pesquisar se as favas da planta causam malformações semelhantes às observas em um dos bezerros nascidos vivos.

To evaluate the toxicity of different concentrations of pods of Stryphnodendron fissuratum to pregnant cows, the pods of this tree were grounded, mixed in a commercial food and given to eight pregnant cows in total doses of 6.5g/kg, 7.5g/kg, 9g/kg and 10g/kg. The animals that received doses of 6.5g/kg delivered normal calves and those that received 7.5g/kg delivered weak calves that did not survive. Doses of 9g/kg resulted in the birth of an immature calf and another with congenital bilateral distichiasis, corneal opacity, and microphthalmia. Both cows that ingested 10g/kg died, and one of these aborted before death. In the dead cows, the gross and histological lesions of the digestive system and liver were similar to those previously described in S. fissuratum poisoning. No significant lesions were observed in the calves and in the aborted fetus. The phytochemical analysis of methanol extracts from pods of S. fissuratum revealed the presence of soluble tannins, proanthocyanidins, leucoanthocyanidins and the triterpenoid saponin β-amyrin. Triterpenoid saponins had been associated with the toxicity of Stryphnodendron spp. and Enterolobium spp., which cause clinical signs similar to those observed in the poisoning by S. fissuratum. The results presented herein confirmed the toxicity of S. fissuratum to bovines. However, the abortive effects of this plant was not confirmed; thus because the abortion and neonatal deaths could be due to the toxicity of the pods to the cows. New research should be done to demonstrate if S. fissuratum is a cause of malformations similar to those observed in one of the calves born from the treated cows.

Aloe ferox Mill., Xanthorrhoeaceae, resin is the solid residue obtained by evaporating the latex that drains from the leaves transversally cut. Aloe ferox has been used in folk medicine as anti-inflammatory, immunostimulant, anti-bacterial, anti-fungal, antitumor, laxative and to heal wounds and burns. The effects of the oral administration of A. ferox resin (10, 25, 50, 100 and 200 mg/kg) were evaluated on intestinal transit in mice and its acute toxicity (5.0 g/kg) in Wistar rats. The hydroxyanthracene derivatives present in the resin were expressed as aloin, identified by thin layer chromatography and quantified by spectrophotometry. The aloin (Rf 0.35) was identified and the percentage of hydroxyanthracene derivates expressed as aloin was 33.5%. A. ferox resin extract (50, 100 and 200 mg/kg) increased the gastrointestinal motility at a 30 min interval at 93.5, 91.8 and 93.8%, respectively, when compared to control group (46.5%). A single oral dose of the A. ferox resin extract did not induce signs of toxicity or death. Thus, the results demonstrate that A. ferox has laxative activity and that it is nontoxic, since LD50 could not be estimated and it is possibly higher than 5.0 g/kg.

O óleo essencial de Schinus terebinthifolius foi analisado por CG e CG-EM. α-Fencheno, limoneno, β-pineno, α-felandreno e β-isosilvestreno representam aproximadamente 80% da composição do óleo. A toxicidade na reprodução de ratos Wistar machos foi avaliada. Não foram observadas mudanças na massa dos órgãos reprodutivos, no número e morfologia dos espermatozoides, nas taxas de reprodução e na massa corporal dos ratos machos após tratamento com o óleo essencial de S. terebinthifolius.

The essential oil of Schinus terebinthifolius (Anacardiaceae) was analyzed by GC and GC-MS. α-Fenchene, limonene, β-pinene, α-phellandrene, and β-isosylvestrene represent about 80% of the oil composition. The reproductive toxicity of the essential oil in Wistar male rats was evaluated. No changes were observed in the mass of the reproductive organs, number and morphology of spermatozoa, reproductive rates, and the body mass of offspring of male rats after treatment with the essential oil of S. terebinthifolius.

The arguments for the usage of the names Gnathoplax, Roeboexodon, R. geryi, and R. guyanensis are revised. Based on the literature and museum specimens, we recommend that the neotype of Exodon guyanensis should be considered valid; that the genus Gnathoplax should be considered an objective junior synonym of Roeboexodon; and that Roeboexodon geryi should be considered an objective junior synonym of Exodonguyanensis.

Os argumentos para o uso dos nomes Gnathoplax, Roeboexodon, R. geryi e R. guyanensis são reavaliados. Baseados na literatura e em espécimes de museu, recomendamos que o neótipo de Exodonguyanensis seja considerado válido, que o gênero Gnathoplax seja considerado sinônimo objetivo júnior de Roeboexodon e que Roeboexodon geryi seja considerado sinônimo objetivo júnior de Exodon guyanensis.

Os incidentalomas adrenais não são infreqüentes e podem ser encontrados em pacientes com hirsutismo. Nesse relato, apresentamos o caso de coexistência de um incidentaloma adrenal com hipertecose de ovário, em uma mulher com 54 anos de idade com amenorréia e hirsutismo de início abrupto e sinais leves de virilização. As testosteronas total e livre basal foram de 191 ng/dL e 179 pmol/L, respectivamente. O ultra-som pélvico demonstrou o ovário direito com 10,3 cc e ovário esquerdo com 9,8 cc, sem nódulos ou cistos e a tomografia computadorizada de abdome demonstrou adrenal direita adrenal e nódulo sólido de 0,8 cm na adrenal esquerda. Após a administração de análogo de GnRH, as testosteronas total e livre foram de 23 ng/dL e 17 pmol/L, respectivamente. Considerando a supressão da concentração de testosterona pelo análogo de GnRH, a paciente foi submetida a histeroooforectomia por via laparoscópica. O diagnóstico histológico foi de hipertecose, com focos de células estromais luteinizadas. Somente folículos atréticos foram visualizados. Não se detectou hiperplasia de células hilares. Em conclusão, a presença de massa adrenal em uma paciente com hirsutismo pode levar ao diagnóstico errado. Neste caso, o teste de supressão com análogo de GnRH foi fundamental para se determinar a origem da hiperandrogenemia.

Adrenal incidentaloma is not infrequent and can be found in hirsute women. We report a case of a 54-year-old woman with amenorrhea and hirsutism of abrupt onset and mild signs of virilization that had an adrenal incidentaloma coexisting with ovarian hyperthecosis. Basal total and free testosterone were 191 ng/dL and 179 pmol/L. Pelvic ultrasonography disclosed a right ovary with 10.3 cc and a left ovary with 9.8 cc without nodules or cysts, and computerized tomography of the abdomen disclosed a normal right adrenal gland. On the left adrenal gland a solid nodule with 0.8 cm was seen. After GnRHa administration, total testosterone was 23 ng/dL and free testosterone was 17 pmol/L. In view of a suppression of testosterone by GnRHa, the patient was submitted to a hystero-oophorectomy by laparoscopy. Symmetrically enlarged ovaries were seen. No tumor was apparent. Histology showed hyperthecosis, with foci of luteinized stromal cells. Only atretic follicles were detected. No hilar cell hyperplasia was seen. In conclusion, the presence of an adrenal mass in a hirsute woman can lead to a wrong diagnosis. In this case the suppression GnRHa test was fundamental to determine the origin of hyperandrogenemia.

OBJETIVO: Investigar uma correlação entre o teste de reatividade da artéria braquial (BART) e o espessamento médio-intimal (EMI) da carótida em uma população de pacientes com doença arterial coronariana, assim como avaliar uma correlação do BART e do EMI da carótida com a gravidade da doença arterial coronariana demonstrada através da coronariografia. MÉTODOS: Quarenta e dois pacientes (idade: 60,7 ± 9,2 anos, 66,7% do sexo masculino) com doença arterial coronariana por coronariografia foram estudados. A função endotelial foi avaliada de modo não-invasivo através do BART, quando foi medido o porcentual de dilatação mediada pelo fluxo (%DMF). O EMI de carótida foi avaliado por meio de ultra-som vascular. RESULTADOS: A média de %DMF foi de 4,7 ± 3,6 e a média de EMI de carótida foi de 1,08 ± 0,23 mm. As medidas do EMI de carótida e do %DMF apresentaram correlação estatisticamente significativa, com coeficiente de Spearman de -0,315, valor p = 0,042, demonstrando que valores menores de %DMF se correlacionaram a um maior EMI de carótida. Não houve correlação entre %DMF, EMI e a gravidade das lesões; CONCLUSÃO: A presença de uma correlação entre o %DMF e o EMI da carótida demonstra a concomitância de alterações vasculares funcionais e anatômicas na doença arterial coronariana, independentemente da gravidade das lesões ateroscleróticas.

OBJECTIVE: To investigate the correlation between the endothelial function and the carotid intimal-medial thickening (IMT) in a population of patients with coronary artery disease, as well as that between the endothelial function and carotid IMT with the severity of the coronary lesions. METHODS: Forty-three patients aged 60.5±9.2 years, (67.4% males) with coronary artery disease at the coronariography were studied. Endothelial function was assessed using the brachial artery reactivity test (BART), which measured the percentage of flow-mediated dilatation (%FMD). The carotid IMT was evaluated through vascular ultrasound. RESULTS: The mean %FDM was 4.7 ± 3.6 and the mean carotid IMT was 1.08 ± 0.23 mm. The carotid MIT and %FMD measurements showed a statistically significant correlation, with Spearman’s coefficient of 0.315, p= 0.042, demonstrating that lower %FMD values corresponded to an increased carotid IMT (r = -0.315, p = 0.042). There was no correlation between %FMD or IMT and the severity of coronary lesions. CONCLUSIONS: The presence of a correlation between carotid IMT and %FMD demonstrates a concomitance of anatomical and functional vascular alterations in coronary artery disease, regardless of the severity of the atherosclerotic lesions.

Composite films were studied as possible candidates for the central or support layer of synthetic paper in a multilayer structure. Recycled post-consumer polypropylene films were reinforced with inorganic fillers at various compositions and under several processing conditions, with the aim of optimizing the physical and mechanical properties of rigidity and low density. Three types of CaCO3, with and without surface treatment of the particles, were used, but only the treated ones were suitable for use in paper films. These samples were then used to analyze possible correlations of properties with composition and processing conditions, varying the CaCO3 particle size distribution and the film processing method, from casting extrusion (flat die) to blown-film extrusion (tubular die). An increase in film stiffness was observed as a function of CaCO3 content and a concentration of 30% CaCO3 was found to be best for the specific application. The flat films were stiffer than the tubular ones. The densities of all the composite films were considered high, compared to a pulp-based paper and a commercial synthetic paper. No significant effect on the physical-mechanical properties analyzed was observed when the CaCO3 particle size distribution was varied. Microcavities were found to form at the surface of flat films submitted to a bi-orientation process performed at laboratory scale; no other sample showed this surface morphology.

Descrevemos aqui uma nova interpretação para a espectros de banda larga da síntese estereosseletiva de antibióticos de adutos Baylis-Hillman. A estrategia é baseada na preparação de um eno-carbamato diretamente do aduto Baylis-Hillman, usando um rearranjo de Curtius. A hidroboração estereosseletiva fornece uma mistura de aminoalcools diasteroisomeros (syn e anti). Após separação cromatográfica, o diasteroisomero syn foi diretamente transformado no antibiótico.

We describe herein a new approach for the stereoselective synthesis of broad spectrum antibiotics from Baylis-Hillman adducts. The strategy is based on the preparation of an ene-carbamate directly from a Baylis-Hillman adduct using a Curtius rearrangement reaction. Stereoselective hydroboration furnished a mixture of diastereoisomeric aminoalcohols (syn and anti). After chromatographic separation, the syn diastereoisomer was directly transformed into the antibiotics.

Descrevemos aqui uma nova interpretação para a espectros de banda larga da síntese estereos-seletiva de antibióticos de adutos Baylis-Hillman. А estrategia é baseada na preparação de um eno-carbamato diretamente do aduto Baylis-Hillman, usando um rearranjo de Curtius. А hidroboração estereosseletiva fornece uma mistura de aminoalcools diasteroisomeros (syn e anti). Após separação cromatográfica, o diasteroisomero syn foi diretamente transformado no antibiótico.

We describe herein a new approach for the stereoselective synthesis of broad spectrum antibiotics from Baylis-Hillman adducts. The strategy is based on the preparation of an ene-carbamate directly from a Baylis-Hillman adduct using a Curtius rearrangement reaction. Stereoselective hydroboration furnished a mixture of diastereoisomeric aminoalcohols (syn and anti). After chromatographic separation, the syn diastereoisomer was directly transformed into the antibiotics.

Três novas espécies do gênero Hyphessobrycon (Characiformes: Characidae) são descritas para a bacia do alto rio Araguaia. Hyphessobrycon langeanii n.sp. se distingue de seus congêneres pela presença de uma mancha umeral redonda e bem definida, de um padrão reticulado de colorido, de uma mancha no pedúnculo caudal horizontalmente alongada e de uma faixa longitudinal larga e difusa. Hyphessobrycon eilyos n.sp. se distingue de seus congêneres pela ausência de manchas umeral e caudal, pela presença de numerosos cromatóforos escuros nas laterais do corpo, mais concentrado na porção ventral da origem da nadadeira pélvica até o final da base da nadadeira anal, pela cor carmim nas nadadeiras dorsal, adiposa e caudal em exemplares vivos, e pela presença de 7-11 dentes maxilares. Hyphessobrycon weitzmanorum n.sp. se distingue de seus congêneres pela presença de duas manchas umerais, por um padrão geral do corpo escuro. Estas três espécies, em conjunto com Creagrutus molinus (Characidae), Apareiodon tigrinus (Parodontidae), uma espécie não descrita de Hypoptopomatinae (Loricariidae), Aspidoras velites (Callichthyidae), Cnesterodon septentrionalis (Poeciliidae) e Simpsonichthys cholopteyx (Rivulidae), todas as quais aparentemente endêmicas do alto rio Araguaia, indicam que esta área trata-se de uma área de endemismo previamente não reconhecida.

Three new species of Hyphessobrycon (Characiformes: Characidae) are described from the upper rio Araguaia basin. Hyphessobrycon langeanii n. sp. is distinguished from all congeners by the presence of a well-defined, round humeral spot, a reticulate color pattern, a broad, horizontally-elongate caudal-peduncle blotch, and a relatively wide, faint midlateral dark stripe. Hyphessobrycon eilyos n. sp. is distinguished from all congeners by the absence of humeral and caudal spots; by the presence of numerous dark chromatophores on the lateral surface of the body, intensely concentrated on the ventral region from the pelvic-fin origin to the end of the caudal-fin base, dorsal, adipose, and caudal fins with carmine red pigmentation in life; and the presence of 7-11 maxillary teeth. Hyphessobrycon weitzmanorum n. sp. is distinguished from all congeners by the combination of the possession of two humeral spots and a general dark color pattern. These three new species, along with Creagrutus molinus (Characidae), Apareiodon tigrinus (Parodontidae), Aspidoras velites (Callichthyidae), an undescribed member of the Hypoptopomatinae (Loricariidae), Cnesterodon septentrionalis (Poeciliidae), and Simpsonichthys cholopteryx (Rivulidae), all of which are apparently endemic of the upper rio Araguaia, indicate that this area is a previously unrecognized area of endemism.

A partir do fracionamento em coluna de gel de sílica do extrato clorofórmico de Polygala paniculata (Polygalaceae), foram isolados 7-metóxi-8-(1',2'-epóxi-3'-metil-3'-butenil)-cumarina (1) e dois artefatos cumarínicos (2a-2b), formados a partir da abertura do anel epóxido de 1 durante o processo de isolamento. O tratamento de 1 com EtOH/SiO2, sob agitação e à temperatura ambiente durante 24 horas, resultou na formação dos respectivos artefatos: 7-metóxi-8-(1'-hidróxi-2-etóxi-3'-metil-3'-butenil)-cumarina (2a) e 7-metóxi-8-(1'-etóxi-2-hidróxi-3'-metil-3'-butenil)-cumarina (2b). As estruturas químicas desses compostos foram determinadas através da análise de seus dados espectrais, incluindo RMN bidimensional.

Fractionation of a chloroform extract of Polygala paniculata (Polygalaceae) on silica gel column chromatography yielded 7-methoxy-8-(1',2'-epoxy-3'-methyl-3'-butenyl)-coumarin (1) and two coumarinic artifacts (2a-2b). The reaction of 1 with EtOH/SiO2 at room temperature for 24 hours yielded 7-methoxy-8-(1'-hydroxy-2'-ethoxy-3'-methyl-3'-butenyl)-coumarin (2a) and 7-methoxy-8-(1'-ethoxy-2'-hydroxy-3'-methyl-3'-butenyl)-coumarin (2b). The structures have been determined by spectral data, including 2D NMR experiments.